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ZSM-5 molecular sieve and preparation method thereof

A ZSM-5, molecular sieve technology, applied in nanotechnology, nanotechnology for materials and surface science, nanotechnology, etc., can solve the problem of difficult separation of crystallization product and reaction medium liquid, single-pot yield limitation, crystallization Long time and other problems, to avoid emissions, save raw material costs, reduce losses

Active Publication Date: 2015-08-19
INST OF PROCESS ENG CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in this method, the crystallization process must be carried out in an aqueous solution, the particle size of the product is large, and the crystallization time is long, the single-pot yield is greatly limited; and the obtained crystallization product is not easy to separate from the liquid phase of the reaction medium

Method used

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  • ZSM-5 molecular sieve and preparation method thereof
  • ZSM-5 molecular sieve and preparation method thereof
  • ZSM-5 molecular sieve and preparation method thereof

Examples

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Embodiment 1

[0084] A kind of preparation method of ZSM-5 molecular sieve, described method is silicon-aluminum source with amorphous silicon dioxide and boehmite, specifically comprises the following steps:

[0085] (1) Homogenization of ingredients: mixing and homogenizing amorphous silica, boehmite and tetrapropylammonium hydroxide (TPAOH) to obtain a ZSM-5 molecular sieve precursor, in which SiO 2 :Al 2 o 3 :TPAOH (substance ratio) is 1:0.01:0.07;

[0086] (2) Assisted crystallization: place a TPAOH aqueous solution with a concentration of 10.5wt% at the bottom of the crystallization tank, place the ZSM-5 molecular sieve precursor obtained in step (1) in the crystallization tank without direct contact with the TPAOH aqueous solution; The mass ratio of the precursor to the TPAOH aqueous solution is 0.1, and the temperature is raised to 190°C for steam-assisted crystallization for 3 hours to obtain the crystallized product, namely ammonium ZSM-5 molecular sieve;

[0087] (3) The ammon...

Embodiment 2

[0090] A preparation method of ZSM-5 molecular sieve, said method uses fumed silica (white carbon black) and aluminum sulfate as silicon and aluminum sources, specifically comprising the following steps:

[0091] (1) Homogenization of ingredients: Mix and homogenize fumed silica (white carbon black), aluminum sulfate and diethylamine (DEN) to obtain a ZSM-5 molecular sieve precursor, in which SiO 2 :Al 2 o 3 :DEN (substance ratio) is 1:0.09:0.15;

[0092] (2) Assisted crystallization: place a DEN aqueous solution with a concentration of 30wt% at the bottom of the crystallization tank, and place the ZSM-5 molecular sieve precursor obtained in step (1) in the crystallization tank without direct contact with the DEN aqueous solution; The mass ratio of the precursor to the DEN aqueous solution was 0.3, and the temperature was raised to 190° C. for steam-assisted crystallization for 50 hours to obtain the crystallized product, namely ammonium ZSM-5 molecular sieve.

[0093] The ...

Embodiment 3

[0095] A kind of preparation method of ZSM-5 molecular sieve, described method is to use embodiment 2 to prepare the DEN solution after ZSM-5 molecular sieve, continue to put a new batch of ZSM-5 molecular sieve precursor (proportioning is the same as embodiment 2) in The crystallization kettle is not in direct contact with the DEN aqueous solution, and the mass ratio of the ZSM-5 molecular sieve precursor to the DEN aqueous solution is 0.5; the temperature is raised to 190°C for steam-assisted crystallization for 5 hours, and the crystallized product is obtained, which is the ammonium ZSM- 5 molecular sieves. The obtained hydrogen ZSM-5 molecular sieve has a particle size of about 40-60nm and a crystallinity of 94.0%.

[0096] Optionally, the templating agent solution can be removed and retained for continued recycling.

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Abstract

The invention relates to a preparation method of a ZSM-5 molecular sieve. The method comprises performing assistant crystallization of a ZSM-5 molecular sieve precursor by utilizing steam of a template agent solution to obtain an ammonium-type ZSM-5 molecular sieve; and optionally, removing the template agent from the ammonium-type ZSM-5 molecular sieve to obtain a hydrogen-type ZSM-5 molecular sieve. According to the invention, the preparation method of the ZSM-5 molecular sieve abandons a conventional continuous medium in a crystallization process, and alkali metals or hydroxides of alkali metals, overcomes the technical prejudice in the prior art, and provides a novel synthesis idea for the field.

Description

technical field [0001] The invention relates to a ZSM-5 molecular sieve and a preparation method thereof, and further relates to an ammonium type ZSM-5 molecular sieve and / or a hydrogen type ZSM-5 molecular sieve and a preparation method thereof. Background technique [0002] ZSM-5 molecular sieve was first reported by Mobil in 1972. It is a five-membered ring zeolite. Its basic structural unit is composed of 8 five-membered rings. This basic structural unit is connected into a chain structure through oxygen bridges, and then Surrounded by a zeolite framework, it has a two-dimensional 10×10 ring channel structure (0.56nm×0.53nm and 0.55nm×0.51nm). ZSM-5 zeolite has become an important catalytic material due to its unique pore structure and acidity, and has been widely used in organic catalytic reactions. ZSM-5 zeolite with small grain size shows good catalytic performance in catalytic reaction, therefore, it is necessary to develop small grain size ZSM-5 zeolite especially ...

Claims

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Application Information

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IPC IPC(8): C01B39/40B82Y30/00B82Y40/00
Inventor 卢旭晨王体壮潘锋
Owner INST OF PROCESS ENG CHINESE ACAD OF SCI
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